CN115007067B - Device and method for preparing high-purity monocrystalline diamond piece - Google Patents

Device and method for preparing high-purity monocrystalline diamond piece Download PDF

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Publication number
CN115007067B
CN115007067B CN202210668968.6A CN202210668968A CN115007067B CN 115007067 B CN115007067 B CN 115007067B CN 202210668968 A CN202210668968 A CN 202210668968A CN 115007067 B CN115007067 B CN 115007067B
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box
motor
pressurizing
compression
paraffin
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CN115007067A (en
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满卫东
龚闯
蒋梅荣
杨春梅
范冰庆
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Shanghai Zhengshi Technology Co Ltd
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Shanghai Zhengshi Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a device and a method for preparing high-purity monocrystalline diamond slices, and belongs to the technical field of artificial diamond manufacturing. The device comprises a pressurizing shell, wherein a first material injection port and a second material injection port are arranged in the pressurizing shell, the first material injection port and the second material injection port are respectively connected with a drying box, the drying box is in sliding contact with a conveying track, a plurality of wax box accommodating grooves are formed in the conveying track, a wax box manufacturing bin is arranged above the conveying track and in the pressurizing shell, a pressurizing cavity is formed in the pressurizing shell, a top pressure component is arranged in the pressurizing cavity, the pressurizing cavity is connected with the drying box through a heat exchange pipeline, a temperature controller is arranged on the heat exchange pipeline, a crushing box is arranged on one side of the pressurizing shell, and the drying box, the conveying track and the top pressure component are connected with a control panel through wires.

Description

Device and method for preparing high-purity monocrystalline diamond piece
Technical Field
The invention relates to the technical field of artificial diamond manufacturing, in particular to a device and a method for preparing high-purity monocrystalline diamond chips.
Background
With the application of diamond in many aspects, the demand of people for diamond is gradually increased, so the exploitation force of diamond is also gradually increased, the content of natural diamond resources is limited, the demand of diamond resources is not required for the current environment, and the environment is irreparable due to excessive development, so people start to try to develop artificial diamond, the performance and purity of the artificial diamond are not equal to those of natural diamond, and the performance of the artificial diamond is different from those of natural diamond, even the strength of some artificial diamond is higher than that of natural diamond, so the development prospect of the artificial diamond is quite considerable, and the devices and equipment manufactured in relation to the artificial diamond are also gradually increased.
Many devices for manufacturing artificial diamonds are available, but the devices have many defects, for example, some devices often cause shaped products to appear in abnormal shapes, and pressure-formed objects caused by uneven objects to be pressed often appear to crack when the pressure is applied, so that the problem that the diamond cannot be formed is caused, meanwhile, some products are not mature in the process, and meanwhile, during the processing, synthetic materials are required to be manually filled, the problems that the specifications and components of the synthetic diamond cannot reach standards due to different proportions of the synthetic materials are caused, and the like are caused frequently, and meanwhile, the problems that the surface cleaning of the formed diamond is incomplete, the cleaning process is complex and the like are also caused frequently in the reproduction process.
Disclosure of Invention
The invention provides a device and a method for preparing high-purity monocrystalline diamond slices, which can effectively solve the problems in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the device includes the pressurization casing, be provided with on the pressurization casing and be provided with first notes material mouth and second notes material mouth, first notes material mouth, the second notes material mouth is connected with the stoving case respectively, stoving case and transportation track sliding contact, be provided with a plurality of wax box mounting groove on the transportation track, the transportation track top is provided with wax box preparation storehouse, wax box preparation storehouse sets up in the pressurization casing, be provided with the pressurization cavity in the pressurization cavity, be provided with the roof pressure subassembly in the pressurization cavity, the pressurization cavity passes through the heat transfer pipeline with the stoving case and is connected, be provided with the temperature controller on the heat transfer pipeline, pressurization casing one side is provided with crushing case, the stoving case, transportation track, roof pressure subassembly passes through the wire and is connected with control panel, first notes material mouth and second notes material mouth respectively add synthetic catalyst and ferroboron alloy, the proportion of synthetic material is controlled more easily to be followed by the stoving case operation, after the stoving is accomplished, add in the paraffin box that is equipped with the carbon sheet, transport track transports the pressurization cavity, wax box preparation storehouse will seal paraffin box in the pressurization cavity, finally will carry out the lid by roof pressure subassembly, after the high-pressure heat transfer is carried out to the paraffin box, will be heated up the heat when will be added to the high temperature heat to the heat transfer pipeline, will be used for the subsequent heat to the heat collecting process of drying.
The drying box is internally provided with a drying table, a first material injection port and a second material injection port are arranged above the drying table, the drying table comprises a main drying table and an auxiliary drying table, the main drying table is rotationally connected with the auxiliary drying table, the main drying table is in sliding connection with a pressurizing shell, the auxiliary drying table is connected with an output end of a drying motor, one side of the auxiliary drying table, which is close to the main drying table, is provided with a fluctuation track, a plurality of connecting struts are arranged on the main drying table, the connecting struts are embedded into the fluctuation track and are in sliding contact with the fluctuation track, the auxiliary drying table is in sliding contact with the transportation track, a telescopic cover is arranged on the auxiliary drying table, the telescopic cover is in sliding connection with the auxiliary drying table through a spring, the upper surface of the main drying table is a conical surface, the upper surface of the auxiliary drying table is an inclined surface with an angle, the auxiliary drying table rotates, and under the action of the fluctuation track and the connecting struts, the main drying table can produce regular vibration, so that the composite material can be well mixed, the efficiency of drying is also increased, the material after the vibration is continuously, the material after the drying uniformly falls on the edge of the auxiliary drying table, the telescopic cover is discharged outside the drying table, and the amount of hands is controlled by the telescopic cover.
The transportation track comprises a transportation hydraulic rod, a cylinder body part of the transportation hydraulic rod is connected with a pressurizing shell, the output end of the transportation hydraulic rod is connected with a transportation plate, a wax box placement groove is arranged on the transportation plate, a travelling motor is arranged below the wax box placement groove, a sliding groove is arranged on the transportation plate, teeth are arranged in the sliding groove, the output end of the travelling motor is meshed with the teeth in the sliding groove, an allocation motor is arranged on the transportation plate, an allocation handle is arranged at the output end of the allocation motor, the allocation handle is arranged at one end of the transportation plate, a material conveying groove is arranged on the allocation handle, one side of the material conveying groove, which is far away from the allocation motor, is propped against a telescopic cover, one side of the material conveying groove, which is close to the allocation motor, is in sliding contact with the wax box placement groove, and after the wax box manufacturing bin is used for manufacturing the wax box, the formed paraffin box is sent to the paraffin box accommodating groove, the paraffin box accommodating groove moves in the sliding groove under the operation of the free motor, the free motor is a servo motor, the position of the paraffin box can be accurately controlled, meanwhile, a manufactured carbon sheet is arranged in the paraffin box and used for forming diamonds, the free motor conveys the paraffin box accommodating groove to the vicinity of the drying table, then the split motor drives the split handle to rotate, the conveying groove props against the telescopic cover, the synthetic material enters the paraffin box from the telescopic cover, then the filled paraffin box is subjected to sealing operation by the paraffin manufacturing bin, and the paraffin box with the sealed cover is conveyed into the top pressing assembly of the pressurizing chamber.
The jacking component comprises a compression hydraulic rod, the compression hydraulic rod is arranged in a compression shell, a jacking head is arranged at the upper output end of the compression hydraulic rod, a pressurizing table is arranged below the jacking head, a lifting hydraulic rod is arranged in the pressurizing table, a first heating plate is arranged on the lifting hydraulic rod, a pressurizing frame is arranged on the pressurizing table, the pressurizing frame comprises two pressurizing plates and two telescopic plates, the two telescopic plates are connected through the telescopic plates, each telescopic plate is in sliding connection with the pressurizing plate, a rotary screw rod is arranged between the pressurizing frame, the rotary screw rod is connected with the compression shell through a locking motor, two sides of the rotary screw rod are respectively provided with opposite screw directions, each pressurizing plate is respectively meshed with two sides of the rotary screw rod, each telescopic plate is respectively connected with the compression shell through the sliding hydraulic rod, a catcher is arranged at one end of the pressurizing table, which is close to the conveying plate, when the catcher sends the paraffin box to the pressurizing table, the pressurizing frame starts to shrink, the locking motor drives the rotating screw rod to rotate, the rotating screw rod is matched with unique bidirectional threads to drive the two pressurizing plates to mutually approach, the sliding hydraulic rods on two sides of the telescopic plates can push the telescopic plates to synchronously approach each other, at the moment, the compression hydraulic cylinders can drive the jacking heads to move downwards, the jacking heads heat in the moving process, the lifting hydraulic rods also synchronously move upwards, the first heating plate heats the paraffin box, the compression distance is adjusted according to specific requirements, the effect of high temperature and high pressure is realized, meanwhile, the fully covered structure is adopted, the paraffin box can not easily generate irregular deformation, the safety of internal synthetic materials is ensured, the problem of synthesis failure is avoided, the specification of the pressurizing frame can be adjusted, the flexibility of the pressurizing process is higher, adapting to more types of synthesis.
The catcher comprises a catching motor, the catching motor is arranged on a pressurizing table, a catching frame is arranged on the catching motor, one end of the catching frame is fixedly connected with the output end of the catching motor, a paraffin ring is arranged at one end of the catching frame, which is far away from the catching motor, one end of the paraffin ring is fixedly connected with the catching frame, one end of the paraffin ring is far away from the catching frame, which is fixedly connected with a contraction spring, the contraction spring is arranged in the catching frame, the contraction spring is connected with a control panel through a wire, the catching motor is driven to work so as to drive the catching frame to rotate, when the paraffin box is sent to one end of the pressurizing table, the catching frame can grasp the paraffin box, the paraffin ring is sleeved on the paraffin box, then the contraction spring of the control panel is supplied with power, the contraction spring is electrified to contract, the paraffin box is clamped, then the catching motor can transfer the paraffin box to the pressurizing table, then the contraction spring is powered off, the paraffin ring is loosened, and the paraffin box can stably fall on the pressurizing table.
The top pressure head includes the top pressure shell, top pressure shell is connected with compression hydraulic stem output, be provided with ultrasonic assembly in the top pressure shell, ultrasonic assembly below is provided with the thermal insulation cover, the thermal insulation cover below is provided with the second hot plate, be provided with a plurality of and touch the probe on the second hot plate, after the second hot plate supports the paraffin box, the second hot plate will carry out the heating operation, ultrasonic assembly will work simultaneously in the heating process, the ultrasonic wave will be by the probe that bumps into the paraffin box, make inside produce vibrations, make the material in the paraffin box obtain abundant mixing, high-speed vibrations also can dissolve some hidden spaces simultaneously, make impurity such as inside air get rid of the paraffin box more rapidly more completely, reduce the influence to synthetic diamond.
Crushing chamber is provided with in the crushing case, be provided with crushing motor in the crushing chamber, be provided with crushing stick on the crushing motor output, be provided with the electro-magnet in the crushing stick, the bottom is provided with the discharge gate in the crushing chamber, be provided with the ejection of compact filter on the discharge gate, ejection of compact filter and discharge gate are detachable construction, crushing chamber passes through the discharge gate and grinding element intercommunication, grinding element sets up at crushing chamber lower extreme, after the fashioned paraffin box enters into crushing case, crushing motor on the crushing case will work, drive crushing stick and rotate, crushing stick will smash fashioned paraffin box, and because the hardness degree of synthetic diamond is higher than crushing stick, synthetic diamond will show out, and deposit on the ejection of compact filter, through dismantling, take out the artifical diamond granule that has been fashioned, the electro-magnet will adsorb the iron-based material after the synthetic, make supplementary crushing effect for smashing the paraffin box simultaneously.
The grinding assembly comprises a grinding box, a grinding disc is arranged in the grinding box, screw threads are arranged on the grinding disc, a grinding brush is arranged above the grinding disc, the grinding brush is arranged on a rotating disc, the grinding brush is connected with the rotating disc through a spring, the rotating disc is rotationally connected with the grinding box through a cleaning motor, a plurality of discharging holes are formed in the grinding disc, crushed materials fall into the grinding box, the rotating disc in the grinding box rotates, the grinding brush is driven to rotate in the rotating process, residues are cleaned by the grinding brush, large-particle substances are extruded in the cleaning process, the grinding box is removed under the action of the grinding disc, the floating washing and other processes are prepared, and the problem of leakage is avoided.
According to the above-mentioned device structure, the method of using the device and the method of producing a single crystal diamond sheet comprise the steps of:
step one: the finished catalyst and ferroboron are mixed in a vibrating way, and then heated and dried at 120-300 ℃ for 4 hours;
step two: preparing a paraffin box, placing a carbon sheet raw material in the paraffin box, and mixing with the dried catalyst and ferroboron;
step three: the top pressing component applies high temperature and high pressure to the paraffin box after the mixing is completed, the temperature is 1000-2300 ℃, the pressure is (50-80) multiplied by 108Pa, and the synthesis time is 1-48h;
step four: crushing the cooled paraffin box, and removing paraffin ash, non-synthesized catalyst and ferroboron alloy to obtain basic synthetic diamond;
step five, a step of performing a step of; and (3) washing the obtained basic diamond for a plurality of times by using distilled water until no obvious impurities exist on the surface.
If the single crystal diamond piece is required to be further purified, the basic diamond can be soaked by adopting strong acid solvents such as concentrated sulfuric acid, concentrated nitric acid and the like, and then the basic diamond is cleaned again until the requirement is met.
Compared with the prior art, the invention has the beneficial effects that: 1. the invention adopts an automatic material conveying manufacturing mode, thereby greatly avoiding uncertain factors caused by interference in the production process, avoiding the problems of re-wetting and the like of the dried synthetic material, and freely controlling the proportion in the production process to finish the effect of automatic material filling and controlling.
2. The invention adopts a comprehensive pressurizing mode instead of the traditional pressurizing mode with specific specification, can ensure that each contact surface can be firmly synthesized in the paraffin box, greatly avoids the problem of damage and leakage caused by uneven stress of the paraffin box, and simultaneously can freely regulate and control the formed shape, so that the final forming effect is more diversified and controllable, and the application range of the device is increased.
3. The invention adopts the unique ultrasonic seam filling structure, can sufficiently eliminate or fill the crack structure in the paraffin box uniformly, ensures that the internal reaction is more sufficient through the vibration of ultrasonic waves, has more obvious contact effect, can disperse the energy of the ultrasonic waves by adopting the synaptic probe, does not cause the problem of overlarge local vibration or overlarge local stress, and greatly improves the yield of products.
4. The invention adopts a heat recovery structure, can fully utilize the waste heat generated during high temperature and high pressure, uses the rest heat for purposes such as material drying, and the like, has adjustable temperature, is more stable and reliable to implement, does not cause waste of energy sources, and greatly reduces the use of the rest energy sources.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a schematic three-dimensional structure of the present invention;
FIG. 2 is a cross-sectional view of the overall structure of the present invention;
FIG. 3 is a schematic view of an assembly structure of a drying table according to the present invention;
FIG. 4 is a schematic view of the internal structure of the transport plate of the present invention;
FIG. 5 is a schematic view of the combination of the pressurizing table and the pressurizing housing of the present invention;
FIG. 6 is a schematic view of the internal structure of the top ram of the present invention;
FIG. 7 is a schematic top view of the press table of the present invention;
FIG. 8 is a schematic view of the structure of the capturing rack according to the present invention;
FIG. 9 is a schematic view of the internal structure of the abrasive assembly of the present invention;
reference numerals in the drawings: 1. a pressurized housing; 2. a first material injection port; 3. a second material injection port; 4. a drying box; 401. a drying table; 402. a main drying table; 403. an auxiliary drying table; 404. a drying motor; 405. a wave track; 406. a connecting strut; 407. a telescoping shield; 5. a transport rail; 501. transporting a transfusion compression bar; 502. a transport plate; 503. a walk-away motor; 504. a sliding groove; 505. the handles are shared; 506. a material conveying groove; 507. a motor is allocated; 6. a wax box placement groove; 7. the wax box manufacturing bin; 8. a pressurizing chamber; 901. compressing the hydraulic rod; 902. a pressing head; 903. a pressurizing table; 904. a lifting hydraulic rod; 905. a first heating plate; 906. pressurizing the frame; 907. a pressurizing plate; 908. a telescoping plate; 909. rotating the lead screw; 910. locking a motor; 911. a sliding hydraulic rod; 912. pressing the shell; 913. an ultrasonic assembly; 914. a thermal insulation cover; 915. a second heating plate; 10. a heat exchange pipeline; 11. a temperature controller; 12. a crushing box; 1201. a pulverizing chamber; 1202. a crushing motor; 1203. crushing the rod; 1204. an electromagnet; 1205. a discharge port; 1206. a discharging filter plate; 13. a catcher; 1301. capturing a motor; 1302. a catching frame; 1303. a paraffin ring; 1304. a retraction spring; 14. a control panel; 15. a grinding assembly; 1501. a grinding box; 1502. a grinding disc; 1503. grinding the hairbrush; 1504. a rotating disc; 1505. and (5) cleaning the motor.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1 to 9, the present invention provides the following technical solutions:
the device includes pressurization casing 1, be provided with on the pressurization casing 1 and be provided with first notes material mouth 2 and second notes material mouth 3, first notes material mouth 2, second notes material mouth 3 are connected with stoving case 4 respectively, stoving case 4 and transportation track 5 sliding contact, be provided with a plurality of wax box mounting groove 6 on the transportation track 5, transportation track 5 top is provided with wax box preparation storehouse 7, wax box preparation storehouse 7 sets up in pressurization casing 1, be provided with the pressurization cavity 8 in the pressurization cavity 8, be provided with the roof pressure subassembly in the pressurization cavity 8 and be connected through heat transfer pipeline 10 with stoving case 4, be provided with accuse material 11 on the heat transfer pipeline 10, be provided with crushing case 12 on one side of pressurization casing 1, stoving case 4, transportation track 5, roof pressure subassembly is connected with control panel 14 through the wire, the proportion of synthetic material of control that adds synthetic and boron iron alloy in first notes material mouth and the second notes material respectively, after the stoving is accomplished, add in the paraffin box that is equipped with the carbon sheet is equipped with to carry out the operation by the stoving, be provided with the pressurization cavity in the transportation track, be provided with the pressurization cavity 8, be provided with the heat transfer cavity in order to avoid the heat transfer cavity to carry out the heat transfer box, can be connected with the heat transfer box and heat transfer pipeline, the heat transfer box is carried out the heat transfer cavity and heat transfer box is carried out, the heat transfer box is heated up, can be connected with the heat transfer cavity and heat transfer box is avoided the heat to the heat transfer box, the heat is lost to the heat is heated, and is finished, the heat can be supplied to the heat transfer box is heated, and the heat to the heat.
The drying box 4 is internally provided with a drying table 401, a first material injection port 2 and a second material injection port 3 are arranged above the drying table 401, the drying table 401 comprises a main drying table 402 and an auxiliary drying table 403, the main drying table 402 is rotationally connected with the auxiliary drying table 403, the main drying table 402 is in sliding connection with the pressurizing shell 1, the auxiliary drying table 403 is connected with the output end of a drying motor 404, one side of the auxiliary drying table 403, which is close to the main drying table 402, is provided with a fluctuation track 405, the main drying table 402, which is close to the auxiliary drying table 403, is provided with a plurality of connecting struts 406, the connecting struts 406 are embedded into the fluctuation track 405 and are in sliding contact with the fluctuation track 405, the auxiliary drying table 403 is in sliding contact with the conveying track 5, a telescopic cover 407 is arranged on the auxiliary drying table 403, the telescopic cover 407 is in sliding connection with the auxiliary drying table 403 through a spring, the upper surface of the main drying table is a conical surface, the upper surface of the auxiliary drying table is an inclined surface with an angle, the auxiliary drying table rotates, and under the action of the fluctuation track and the connecting struts, the auxiliary drying table is regularly vibrated, the composite material is better mixed, meanwhile, the vibration efficiency of the composite material is increased, the vibration material is evenly discharged from the auxiliary drying table via the telescopic cover, and the drying amount is evenly discharged from the drying table through the telescopic cover.
The transportation track 5 comprises a transportation fluid pressure rod 501, a cylinder part of the transportation fluid pressure rod 501 is connected with a pressurizing shell 1, the output end of the transportation fluid pressure rod 501 is connected with a transportation plate 502, a wax box accommodating groove 6 is arranged on the transportation plate 502, a travelling motor 503 is arranged below the wax box accommodating groove 6, a sliding groove 504 is arranged on the transportation plate 502, teeth are arranged in the sliding groove 504, the output end of the travelling motor 503 is meshed with the teeth in the sliding groove 504, an allocation motor 507 is arranged on the transportation plate 502, an allocation handle 505 is arranged on the output end of the allocation motor 507, the allocation handle 505 is arranged at one end of the transportation plate 502, a conveying groove 506 is arranged on the allocation handle 505, one side of the conveying groove 506 is far away from the allocation motor 507, one side of the conveying groove 506 is close to the allocation motor 507 and is in sliding contact with the wax box accommodating groove 6, after the wax box is manufactured, the formed wax box accommodating bin is conveyed onto the wax box accommodating groove, the formed wax box accommodating groove moves in the sliding groove, the travelling motor 503, the travelling motor is meshed with the teeth in the sliding groove, the conveying motor is a servo motor, the split motor is arranged on the sliding groove, the split motor is arranged on the split motor, the split motor 507, the position is arranged on the transport motor, the split motor 507 is arranged on the side of the split motor, the split motor is arranged on the side of the conveying groove, the conveying box is formed into a rotary cover, the box is closed, the split box is formed into a rotary cover, the box, the split box is closed, the split box is pressed into a rotary cover, and the split box is closed, and the split box is pressed, and then, and is pressed into a telescopic box, and is pressed, and then, and is pressed into a telescopic box.
The jacking assembly comprises a compression hydraulic rod 901, the compression hydraulic rod 901 is arranged in a compression shell 1, a jacking head 902 is arranged at the upper output end of the compression hydraulic rod 901, a pressurizing table 903 is arranged below the jacking head 902, a lifting hydraulic rod 904 is arranged in the pressurizing table 903, a first heating plate 905 is arranged on the lifting hydraulic rod 904, a pressurizing frame 906 is arranged on the pressurizing table 903, the pressurizing frame 906 comprises two pressurizing plates 907 and two expansion plates 908, the pressurizing plates 907 are connected through the expansion plates 908, each expansion plate 908 is in sliding connection with the pressurizing plates 907, a rotary screw 909 is arranged between the pressurizing frames 906, the rotary screw 909 is connected with the compression shell 1 through a locking motor 910, two sides of the rotary screw 909 are respectively provided with opposite thread directions, each pressurizing plate 907 is respectively meshed with two sides of the rotary screw 909, each expansion plate 908 is respectively connected with the compression shell 1 through a sliding hydraulic rod 911, the pressing platform 903 is provided with a catcher 13 near one end of the transport plate 502, when the catcher sends the paraffin box to the pressing platform, the pressing frame starts to shrink, the locking motor drives the rotating screw rod to rotate, the rotating screw rod is matched with unique bidirectional threads to drive the two pressing plates to mutually approach, the sliding hydraulic rods on two sides of the telescopic plates can push the telescopic plates to synchronously approach each other, at the moment, the compression hydraulic cylinders can drive the pressing heads to move downwards, the pressing heads heat in the moving process, the lifting hydraulic rods also synchronously move upwards, the first heating plate heats the paraffin box, the compression distance is adjusted according to specific requirements, the effect of high temperature and high pressure is realized, meanwhile, the paraffin box can not easily generate irregular deformation due to the adoption of a fully-covered structure, the safety of internal synthetic materials is ensured, the problem of synthesis failure is avoided, the specification of the pressing frame can be adjusted, the flexibility of the pressurizing process is higher, and the pressurizing process is suitable for more types of synthesis.
The catcher 13 comprises a catching motor 1301, the catching motor 1301 is arranged on a pressurizing table 903, a catching frame 1302 is arranged on the catching motor 1301, one end of the catching frame 1302 is fixedly connected with the output end of the catching motor 1301, a paraffin ring 1303 is arranged at one end of the catching frame 1302, which is far away from the catching motor 1301, one end of the paraffin ring 1303 is fixedly connected with the catching frame 1302, one end of the paraffin ring 1303 is far away from the catching frame 1302 and is fixedly connected with a shrinkage spring 1304, the shrinkage spring 1304 is arranged in the catching frame 1302, the shrinkage spring 1304 is connected with a control panel 14 through a wire, the catching motor works to drive the catching frame to rotate, when the paraffin box is sent to one end of the pressurizing table, the catching frame grabs the paraffin box, the paraffin ring is sleeved on the paraffin box, then the control panel box is powered on, the shrinkage spring is electrified to shrink, the paraffin box is clamped, then the catching motor transfers the paraffin box to the pressurizing table, the shrinkage spring is powered off, the paraffin ring is loosened, and the paraffin box is stably dropped on the pressurizing table.
The top pressure head 902 includes top pressure shell 912, top pressure shell 912 is connected with compression hydraulic stem 901 output, be provided with ultrasonic assembly 913 in the top pressure shell 912, ultrasonic assembly 913 below is provided with thermal insulation cover 914, thermal insulation cover 914 below is provided with second hot plate 915, be provided with a plurality of synaptic probe on the second hot plate 915, after the second hot plate supports the paraffin box, the second hot plate will carry out the heating operation, ultrasonic assembly will work simultaneously in the heating process, the ultrasonic assembly will be scattered into the paraffin box by the synaptic probe, make inside produce vibrations, make the material in the paraffin box obtain abundant mixing, high-speed vibrations also can solve some hidden spaces simultaneously, make impurity such as inside air get rid of the paraffin box more rapidly more completely, reduce the influence to synthetic diamond.
The crushing box 12 is internally provided with a crushing chamber 1201, a crushing motor 1202 is arranged in the crushing chamber 1201, a crushing rod 1203 is arranged at the output end of the crushing motor 1202, an electromagnet 1204 is arranged in the crushing rod 1203, the bottom end in the crushing chamber 1201 is provided with a discharge hole 1205, the discharge hole 1205 is provided with a discharge filter plate 1206, the discharge filter plate 1206 and the discharge hole 1205 are of a detachable structure, the crushing chamber 1201 is communicated with a grinding assembly 15 through the discharge hole 1205, the grinding assembly 15 is arranged at the lower end of the crushing chamber 1201, after a formed paraffin box enters the crushing box, the crushing motor on the crushing box works to drive the crushing rod to rotate, the crushing rod breaks the formed paraffin box, and due to the fact that the hardness degree of synthetic diamond is higher than that of the crushing rod, the synthetic diamond is exposed out and deposited on the discharge filter plate, the formed artificial diamond particles are taken out after the disassembly, and simultaneously the electromagnet also adsorbs the synthesized iron-based substances, and simultaneously the auxiliary crushing effect is achieved for breaking the paraffin box.
The grinding component 15 comprises a grinding box 1501, a grinding disc 1502 is arranged in the grinding box 1501, screw threads are arranged on the grinding disc 1502, a grinding brush 1503 is arranged above the grinding disc 1502, the grinding brush 1503 is arranged on a rotating disc 1504, the grinding brush 1503 is connected with the rotating disc 1504 through springs, the rotating disc 1504 is rotationally connected with the grinding box 1501 through a cleaning motor 1505, a plurality of discharging holes are formed in the grinding disc, crushed materials fall into the grinding box, the rotating disc in the grinding box rotates, the grinding brush is driven to rotate in the rotating process, residues are cleaned by the grinding brush, large-particle substances are extruded in the cleaning process, the grinding box is removed under the action of the grinding disc, the floating washing and other processes are prepared, and the problem of leakage is avoided.
According to the above-mentioned device structure, the method of using the device and the method of producing a single crystal diamond sheet comprise the steps of:
step one: and (3) vibrating and mixing the finished catalyst and ferroboron, and then heating and drying the mixture for 4 hours at the temperature of 120-300 ℃. The catalyst and the ferroboron are sent into a drying box, and the drying box can be subjected to specific control on temperature and time according to specific quality and conditions of the drying box;
step two: preparing a paraffin box, placing a carbon sheet raw material in the paraffin box, and mixing with the dried catalyst and ferroboron;
step three: the top pressing component applies high temperature and high pressure to the paraffin box after the mixing is completed, the temperature is 1000-2300 ℃, the pressure is (50-80) multiplied by 108Pa, and the synthesis time is 1-48h;
step four: crushing the cooled paraffin box, and removing paraffin ash, non-synthesized catalyst and ferroboron alloy to obtain basic synthetic diamond;
step five, a step of performing a step of; and (3) washing the obtained basic diamond for a plurality of times by using distilled water until no obvious impurities exist on the surface.
If the single crystal diamond piece is required to be further purified, the basic diamond can be soaked by adopting strong acid solvents such as concentrated sulfuric acid, concentrated nitric acid and the like, and then the basic diamond is cleaned again until the requirement is met.
The working principle of the invention is as follows: the first material injection port and the second material injection port are respectively added with a synthetic catalyst and ferroboron, then the drying operation is carried out by the drying box, the mutual motion between the main drying table and the auxiliary drying table is achieved, the effect of high-speed vibration is achieved, and the synthetic material is dried by utilizing heat from the pressurizing chamber.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. An apparatus for preparing high purity single crystal diamond chips, characterized in that: the device comprises a pressurizing shell (1), wherein a first material injection port (2) and a second material injection port (3) are arranged in the pressurizing shell (1), the first material injection port (2) and the second material injection port (3) are respectively connected with a drying box (4), the drying box (4) is in sliding contact with a conveying track (5), a plurality of wax box accommodating grooves (6) are formed in the conveying track (5), a wax box manufacturing bin (7) is arranged above the conveying track (5), the wax box manufacturing bin (7) is arranged in the pressurizing shell (1), a pressurizing cavity (8) is arranged in the pressurizing shell (1), a jacking component is arranged in the pressurizing cavity (8), the pressurizing cavity (8) is connected with the drying box (4) through a heat exchange pipeline (10), a temperature controller (11) is arranged on the heat exchange pipeline (10), a smashing box (12) is arranged on one side of the pressurizing shell (1), and the drying box (4), the conveying track (5) and a jacking component are connected with a control panel (14) through wires.
Be provided with stoving platform (401) in stoving case (4), stoving platform (401) top is provided with first notes material mouth (2), second notes material mouth (3), stoving platform (401) include main stoving platform (402) and vice stoving platform (403), main stoving platform (402) and vice stoving platform (403) swivelling joint, main stoving platform (402) and pressurization casing (1) sliding connection, vice stoving platform (403) are connected with stoving motor (404) output, vice stoving platform (403) are provided with undulant track (405) near main stoving platform (402) one side, be provided with a plurality of connection pillar (406) on main stoving platform (402) are close to vice stoving platform (403), connection pillar (406) imbeds into undulant track (405) and with undulant track (405) sliding contact, vice stoving platform (403) are provided with expansion cover (407) on vice stoving platform (403), vice stoving platform (403) and vice stoving platform (403) are through spring sliding connection.
2. An apparatus for producing a high purity single crystal diamond sheet according to claim 1, wherein: transportation track (5) are including transporting infusion depression bar (501), transportation hydraulic pressure pole (501) cylinder body part is connected with pressurization casing (1), transportation hydraulic pressure pole (501) output is connected with transportation board (502), be provided with wax box mounting groove (6) on transportation board (502), wax box mounting groove (6) below is provided with and walks motor (503), set up sliding tray (504) on transportation board (502), be provided with tooth in sliding tray (504), walk motor (503) output and tooth meshing in sliding tray (504), be provided with on transportation board (502) and allocate motor (507), be provided with on the output of allocation motor (507) and allocate silo (505), allocation handle (505) set up in transportation board (502) one end, be provided with on allocation handle (505) and pass silo (506), it supports motor (507) one side expansion cover (407) to keep away from allocation motor (507), it supports to pass silo (507) to be close to allocation silo (6) contact with allocation silo.
3. An apparatus for producing a high purity single crystal diamond sheet according to claim 2, wherein: the jacking assembly comprises a compression hydraulic rod (901), the compression hydraulic rod (901) is arranged in a compression shell (1), a jacking head (902) is arranged at the upper output end of the compression hydraulic rod (901), a compression table (903) is arranged below the jacking head (902), a lifting hydraulic rod (904) is arranged in the compression table (903), a first heating plate (905) is arranged on the lifting hydraulic rod (904), a compression frame (906) is arranged on the compression table (903), the compression frame (906) comprises two compression plates (907) and two expansion plates (908), the compression plates (907) are connected through the expansion plates (908), each expansion plate (908) is in sliding connection with the compression plates (907), a rotary screw rod (909) is arranged between the compression frame (906), the rotary screw rod (909) and the compression shell (1) are connected through a locking motor (910), opposite thread directions are respectively arranged on two sides of the rotary screw rod (909), each compression plate (907) is respectively meshed with the rotary screw rod (907) and each compression plate (908) through the compression plate (908) respectively, the pressurizing table (903) is provided with a catcher (13) near one end of the conveying plate (502).
4. An apparatus for producing a high purity single crystal diamond sheet according to claim 3, wherein: the catcher (13) comprises a catching motor (1301), the catching motor (1301) is arranged on a pressurizing table (903), a catching frame (1302) is arranged on the catching motor (1301), one end of the catching frame (1302) is fixedly connected with the output end of the catching motor (1301), one end of the catching frame (1302) is far away from the catching motor (1301) and is provided with a paraffin ring (1303), one end of the paraffin ring (1303) is fixedly connected with the catching frame (1302), one end of the paraffin ring (1303) is far away from the catching frame (1302) and is fixedly connected with a contraction spring (1304), the contraction spring (1304) is arranged in the catching frame (1302), and the contraction spring (1304) is connected with a control panel (14) through a wire.
5. An apparatus for producing a high purity single crystal diamond sheet according to claim 3, wherein: the pressure head (902) comprises a pressure shell (912), the pressure shell (912) is connected with the output end of the compression hydraulic rod (901), an ultrasonic assembly (913) is arranged in the pressure shell (912), a heat insulation cover (914) is arranged below the ultrasonic assembly (913), a second heating plate (915) is arranged below the heat insulation cover (914), and a plurality of synaptic probes are arranged on the second heating plate (915).
6. An apparatus for producing a high purity single crystal diamond sheet according to claim 1, wherein: crushing chamber (1201) are provided with in crushing case (12), be provided with crushing motor (1202) in crushing chamber (1201), be provided with crushing stick (1203) on crushing motor (1202) output, be provided with electro-magnet (1204) in crushing stick (1203), crushing chamber (1201) inner bottom is provided with discharge gate (1205), be provided with ejection of compact filter (1206) on discharge gate (1205), ejection of compact filter (1206) are detachable construction with discharge gate (1205), crushing chamber (1201) communicate with grinding assembly (15) through discharge gate (1205), grinding assembly (15) set up at crushing chamber (1201) lower extreme.
7. An apparatus for producing a high purity single crystal diamond sheet according to claim 6, wherein: the grinding assembly (15) comprises a grinding box (1501), a grinding disc (1502) is arranged in the grinding box (1501), precession threads are arranged on the grinding disc (1502), a grinding brush (1503) is arranged above the grinding disc (1502), the grinding brush (1503) is arranged on a rotating disc (1504), the grinding brush (1503) is connected with the rotating disc (1504) through a spring, the rotating disc (1504) is connected with the grinding box (1501) in a rotating mode through a cleaning motor (1505), and a plurality of discharging holes are formed in the grinding disc (1502).
8. The method of using an apparatus for producing high purity single crystal diamond chips according to claim 1, wherein: the using method comprises the following steps:
step one: the finished catalyst and ferroboron are mixed in a vibrating way, and then heated and dried at 120-300 ℃ for 4 hours;
step two: preparing a paraffin box, placing a carbon sheet raw material in the paraffin box, and mixing with the dried catalyst and ferroboron;
step three: the top pressing component applies high temperature and high pressure to the paraffin box after the mixing is completed, the temperature is 1000 ℃ to 2300 ℃, and the pressure is (50 to 80) multiplied by 10 8 Pa, and synthesizing time is 1-48h;
step four: crushing the cooled paraffin box, and removing paraffin ash, non-synthesized catalyst and ferroboron alloy to obtain basic synthetic diamond;
step five, a step of performing a step of; and (3) washing the obtained basic diamond for a plurality of times by using distilled water until no obvious impurities exist on the surface.
CN202210668968.6A 2022-06-14 2022-06-14 Device and method for preparing high-purity monocrystalline diamond piece Active CN115007067B (en)

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